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A solid-phase extraction-gas chromatography-tandem mass spectrometry method for the detection of multi-component residues of organophosphorus pesticides in aquatic products

An organophosphorus pesticide and gas chromatography technology, which is applied in the field of aquatic product quality and safety testing, can solve the problems of limited ability and limited effect of removing matrix interferences, and achieve the effect of good impurity removal and purification, rapid analysis and reduction of interference.

Active Publication Date: 2020-07-17
MARINE FISHERIES RES INST OF ZHEJIANG
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the QuEChERS sample pretreatment method is widely used in the analysis of multi-residue pesticides, its ability to remove matrix interferences is limited. It is more suitable for the analysis of vegetable samples with little organic matter, and has limited effect on aquatic products rich in organic matter.

Method used

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  • A solid-phase extraction-gas chromatography-tandem mass spectrometry method for the detection of multi-component residues of organophosphorus pesticides in aquatic products
  • A solid-phase extraction-gas chromatography-tandem mass spectrometry method for the detection of multi-component residues of organophosphorus pesticides in aquatic products
  • A solid-phase extraction-gas chromatography-tandem mass spectrometry method for the detection of multi-component residues of organophosphorus pesticides in aquatic products

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Example 1 Determination of 28 organophosphorus pesticides in grass carp

[0022] Sample solvent extraction: Accurately weigh 5.0g of grass carp sample into a 50mL centrifuge tube, add 5g of anhydrous sodium sulfate and 20mL of acetonitrile / ethyl acetate mixed solvent (1:1 volume ratio) into the centrifuge tube, vortex for 2min, After ultrasonic extraction for 15min, centrifuge at 5000r / min for 5min, filter the supernatant through a column equipped with 10g of anhydrous sodium sulfate into a 100mL rotary evaporator, and wash the residue with 20mL of acetonitrile / ethyl acetate mixed solvent (1:1 volume ratio ) Repeat vortex oscillation and ultrasonic extraction, centrifuge under the same conditions as above, filter the supernatant in the above-mentioned 100mL rotary steamer, thereby combining the extracts;

[0023] (2) SPE column purification: the obtained extract was concentrated to dryness by rotary evaporation in a water bath at 40°C, and 1 mL of n-hexane was added to ...

Embodiment 2

[0028] Determination of 28 kinds of organophosphorus pesticides in embodiment 2 razor clams

[0029] (1) Sample solvent extraction: Accurately weigh 5.0 g of a razor clam sample in a tidal flat into a 50 mL centrifuge tube, add 5 g of anhydrous sodium sulfate and 20 mL of acetonitrile / ethyl acetate mixed solvent (1:1 volume ratio) into the centrifuge tube, Vortex for 2 minutes, after ultrasonic extraction for 15 minutes, centrifuge at 5000 r / min for 5 minutes, filter the supernatant through a column equipped with 10 g of anhydrous sodium sulfate into a 100 mL rotary evaporator, and wash the residue with 20 mL of acetonitrile / ethyl acetate mixed solvent ( 1:1 volume ratio) Repeat vortex oscillation, ultrasonic extraction, centrifuge under the same conditions as above, filter the supernatant into the above 100mL rotary evaporator, and combine the extracts;

[0030] (2) SPE column purification: the obtained extract was concentrated to dryness by rotary evaporation in a water bath...

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Abstract

The invention discloses a method for detecting multi-component organophosphorus pesticide residues in aquatic products by solid-phase extraction-gas chromatography-tandem mass spectrometry. The methodcomprises the following steps of sample solvent extraction to obtain extract liquor, solid-phase extraction and purification to obtain purified liquor, and gas chromatography-tandem mass spectrometrydetection as well as quantification by an external standard method. The method for detecting the multi-component organophosphorus pesticide residues in the aquatic products by solid-phase extraction-gas chromatography-tandem mass spectrometry is convenient to operate, high in reproducibility, accurate in qualification and high in recovery rate. The multi-component organophosphorus pesticide residues in the aquatic products can be analyzed quickly. The method is a convenient and accurate method for detecting organophosphorus pesticides in trace amount in the aquatic products, so as to achievequantitative and qualitative analysis of organophosphorus pesticides in trace amount in the aquatic products.

Description

technical field [0001] The invention relates to the technical field of quality and safety detection of aquatic products, in particular to a method for detecting multi-component residues of organophosphorus pesticides in aquatic products by solid-phase extraction-gas chromatography tandem mass spectrometry. Background technique [0002] Organophosphorus pesticides are a class of pesticides that occupy the largest share in my country's pesticide market and are widely used. In theory, organophosphorus pesticides are considered to be easily degradable, difficult to bioaccumulate, and have less impact on the ecology. They were once considered as substitutes for organochlorine pesticides. [0003] In fact, organophosphorus pesticides can form phosphorylated cholinesterase with cholinesterase in the organism, thereby causing toxicity to the organism. At the beginning of 2010, the "poisonous cowpea" incident caused a sensation throughout the country, and organic phosphorus was dete...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 孙秀梅金衍健郝青胡红美钟志郭远明
Owner MARINE FISHERIES RES INST OF ZHEJIANG